EP3987088B1 - Vorbereitungsmethode und vorrichtung zur herstellung von recycling-faserspinnlösungen unter verwendung der lösungsmittelmethode - Google Patents

Vorbereitungsmethode und vorrichtung zur herstellung von recycling-faserspinnlösungen unter verwendung der lösungsmittelmethode Download PDF

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Publication number
EP3987088B1
EP3987088B1 EP20736252.6A EP20736252A EP3987088B1 EP 3987088 B1 EP3987088 B1 EP 3987088B1 EP 20736252 A EP20736252 A EP 20736252A EP 3987088 B1 EP3987088 B1 EP 3987088B1
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EP
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Prior art keywords
wiped film
kneading reactor
nmmo
film evaporators
vacuum
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EP20736252.6A
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English (en)
French (fr)
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EP3987088C0 (de
EP3987088A1 (de
Inventor
Roland Kunkel
Daniel Witte
Sven KÖNIG
Manuel Steiner
Weilie Wang
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List Technology AG
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List Technology AG
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00—Treatment of filament-forming or like material
    • D01D1/02—Preparation of spinning solutions
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F13/00—Recovery of starting material, waste material or solvents during the manufacture of artificial filaments or the like
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
    • Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear

Definitions

  • the present invention relates to the field of textile technology, and in particular to a method and a device for preparing a regenerated cellulose fiber spinning dope using a solvent method.
  • the solvent method for producing regenerated cellulose fiber solution is mainly prepared by mixing NMMO solvent with cellulose.
  • the preparation process of lyocell fiber solution is now illustrated as an example.
  • the preparation of lyocell fiber solution is a high-viscosity spinnable dope which is dissolved by direct physical modification of cellulose using a non-toxic solvent NMMO (N-methylmorpholine-M-oxide).
  • NMMO N-methylmorpholine-M-oxide
  • the object of the present invention is to provide an improved system and preparation method of a regenerated cellulose fiber spinning dope by a solvent method.
  • the present invention provides a system and a preparation method of a regenerated cellulose fiber spinning dope by a solvent method based on the understanding of the advantages and disadvantages of the above method. It changes the operating process and equipment configuration to achieve a significant increase in single-line capacity while ensuring a better homogenized solvent-based spinning solution. For example, the capacity of each production line can reach 40,000 tons per year, or 60,000 tons per year (330 days).
  • a single set of devices can be configured in combination with two or more (hereinafter collectively referred to as multiple) wiped film evaporators and a single kneading reactor depending on the capacity requirements.
  • the size of the equipment is optimized according to the capacity.
  • Each wiped film evaporator and the kneading reactor are preferably equipped with a separate condensing system.
  • the temperature of the jacketed heat medium of each single device can be adjusted by comparing the actual amount of evaporated water with the theoretical calculated value. Adjusting the rotor rotation number or vacuum adjustment or a combination of both can be used to control the amount of evaporation water, that is, the control of the degree of dissolution of the dope.
  • NMMO solvent As an example: The cellulose suspension containing NMMO is separately injected into a plurality of vertical wiped film evaporators for pre-evaporation, and then the suspension is transported to a horizontal kneading reactor for evaporation and mixing. A homogenized dope is formed and discharged. Based on three known devices, the dissolution process of NMMO-containing cellulose pulp in NMMO was analyzed from a process technology perspective.
  • the dissolution process can be basically divided into three steps.
  • the first step is to evaporate water from the cellulose-solvent pulp until the dissolution starting point of the cellulose. This starting point corresponds to reaching the dissolution window, corresponding to about 2.5 hydrated NMMO. This step requires a large amount of thermal energy to evaporate the water, but since the cellulose has not been dissolved without any additional residence time, and the viscosity of the pulp is low.
  • the main dissolution of the viscosity is significantly increased in the second step. This step evaporates relatively little water and evaporates to about 1.5 hydrated NMMO.
  • the third step is determined by the degree of homogenization of the spinning dope and by evaporation of less water to 0.8 to 1.0 hydrate depending on the concentration of cellulose.
  • An advantage of the present invention is that the device utilizes a good thermal conductivity of the wiped film evaporator to facilitate evaporation of a large amount of moisture in the case where the viscosity is low in the first step and the residence time is short. Due to the low viscosity, the power consumption of the motor is also significantly reduced. Kneading reactor are suitable for the second and third steps due to their excellent homogenization performance and long residence time, as well as the ability to handle high viscosity materials and less water evaporation requirements.
  • Another major advantage of the method and system of the present invention is the high throughput / performance rate, even when compared to known systems containing exactly one wiped film evaporator upstream of exactly one kneading reactor.
  • references number 7 refers to either auger or straight transition
  • reference number 8 refers tor pump or auger or straight transition
  • reference number 9 refers to kneading reactor
  • reference number 10 refers to condensation.
  • the following embodiments illustrate the features and advantages of the present invention by taking two wiped film evaporator corresponding to a kneading reactor as an example; the drawings of the present invention are not unique, and multiple wiped film evaporations can be performed according to customer and capacity requirements.
  • the device corresponds to a kneading reactor for different combinations.
  • Example 1 referring to Figure 1 differs from example 2 / Figure 2 only with respect to the transitions 7, 8 between the wiped film evaporators 3, 4 and the kneading reactor 9. In contrast to example 2, the transitions 7, 8 of example 1 are not combined before entering the kneading reactor 9.
  • Example 2 / Figure 2 The cellulose mixture previously mixed with NMMO and the auxiliary agent was metered into the wiped film evaporators 3 and 4 separately through the input lines 1 and 2, and it was also possible to carry out separately.
  • the connecting sections can be set separately ( Figure 1 ) or concentrated first to one or more main pipes ( Figure 2 ) before being connected to the kneading reactor 9.
  • the injected mixture material is subjected to evaporation and concentration of water.
  • the concentrated material is transferred from the wiped film evaporators 3 and 4 (which can be carried out simultaneously or separately) into the same corresponding kneading reactor 9.
  • the mixture material is formed into a film from the wiped film evaporator and the material is evaporated under vacuum, and the cellulose is evaporated under vacuum. No dissolution was achieved during this process.
  • the material is thoroughly mixed with the solvent (NMMO) and partially evaporated to achieve cellulose dissolution, thereby forming a highly viscous spinnable dope.
  • the spinning dope is then conveyed through a pipe and a pump body to a spinning machine through a discharge device for spinning.
  • cellulose concentration in the dope In order to further increase the productivity, it is also possible to slightly increase the cellulose concentration in the dope, and then dilute it to a suitable spinnable cellulose spinning solution. Dilution is done through the input line in the discharge unit. It may also be diluted upstream of the kneading reactor upstream of the discharge device or dispersed at multiple locations simultaneously.
  • the dope is conveyed downstream of the discharge device by means of one or more pumps to the downstream processing and spinning device.
  • the secondary vapor generated in the wiped film evaporators 3 and 4 and the kneading reactor 9 is condensed by a correspondingly connected condenser.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Artificial Filaments (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Claims (15)

  1. Verfahren zur Herstellung einer regenerierten Zellulosefaser-Spinnlösung durch ein Lösungsmittelverfahren, bei dem ein wässriges Gemisch aus Zellulose und einem Lösungsmittel und einem Hilfsstoff zu einer spinnbaren Zellulose-Spinnlösung verarbeitet wird, dadurch gekennzeichnet, dass das Materialgemisch zunächst in zwei oder mehrere vertikale Wischfilmverdampfer (3, 4) eingetragen wird, dann in einen mit den Wischfilmverdampfern verbundenen horizontalen, vorzugsweise zylindrischen Knetreaktor (9) eingetragen und unter Vakuum verdampft und gemischt wird.
  2. Verfahren nach Anspruch 1, bei dem der Verbindungsabschnitt entweder eine Pumpe oder eine Schnecke zum Fördern des Materials durch die Rohrleitung verwendet, oder wobei der Verbindungsabschnitt ein Schwerkraft-Verfahren für die Materialförderung verwendet oder wobei der Verbindungsabschnitt eine unmittelbare Verbindung bereitstellt.
  3. Verfahren nach Anspruch 1, wobei jeder der einzelnen vertikalen Wischfilmverdampfer (3, 4) und die vorzugsweise zylindrische Knetreaktoreinheit (9) jeweils mit einem separaten Kondensationssystem versehen sind.
  4. Verfahren nach Anspruch 1, wobei das Vakuumsystem jedes der einzelnen vertikalen Wischfilmverdampfer (3, 4) und des vorzugsweise zylindrischen Knetreaktors (9) getrennt oder gemeinsam konfiguriert werden können oder der Wischfilmverdampfer (3, 4) einen Satz von Vakuumsystemen gemeinsam nutzt.
  5. Verfahren nach Anspruch 1, wobei jeder einzelne vertikale Wischfilmverdampfer (3, 4) und vorzugsweise der zylindrische Knetreaktor (9) bei unterschiedlichen Vakuumdrücken oder bei demselben Vakuumdruck arbeitet.
  6. Verfahren nach den Ansprüchen 1-5, dadurch gekennzeichnet, dass das Lösungsmittel NMMO oder ein anderes Lösungsmittel ist, das Zellulose auflösen kann.
  7. Verfahren nach Anspruch 1, bei dem das Gemisch in den vertikalen Wischfilmverdampfern (3, 4) Feuchtigkeit verdampft und die Lösungsmittelkonzentration erhöht, welche jedoch geringer ist als die für die Zelluloseauflösung erforderliche Konzentration.
  8. Verfahren nach Anspruch 7, dadurch gekennzeichnet, dass das NMMO auf ein Niveau oberhalb des Monohydrats konzentriert wird, wobei ein von NMMO dominiertes Lösungsmittel verwendet wird, vorzugsweise ist das Verhältnis von NMMO zu Wasser und NMMO geringer als 86,7%.
  9. Verfahren nach Anspruch 1, wobei in dem Knetreaktor (9) das von den Wischfilmverdampfern (3, 4) zum Knetreaktor (9) geschickte Material die zur Auflösung benötigte Lösungsmittelkonzentration durch Verdampfen von Feuchtigkeit auf den Grad der Auflösung mit Zellulose erhöht, um eine verspinnbare Spinnlösung zu bilden.
  10. Verfahren nach Anspruch 9, bei dem das NMMO auf ein Niveau des Monohydrats, wie z.B. ein auf NMMO basierendes Lösungsmittel, konzentriert wird, wobei vorzugsweise das Verhältnis von NMMO zu Wasser und NMMO nicht weniger als 86,7% beträgt.
  11. Verfahren nach Anspruch 1, wobei die Dampftemperatur im Mantel des der Wischfilmverdampfers (3, 4) zwischen 100-180°C, vorzugsweise 100-150°C, und die Heisswassertemperatur des Mantels 80- 105°C beträgt und das Mantelwärmemedium des Knetreaktors (9) zwischen 90-120°C, vorzugsweise 100-110°C, arbeitet.
  12. Verfahren nach Anspruch 1, wobei die Wischfilmverdampfer (3, 4) und der Knetreaktor (9) unter einem Vakuum von 40-100 mbar, vorzugsweise 45-55 mbar unter Vakuumbetriebsbedingungen betrieben werden.
  13. Verfahren nach Anspruch 12, wobei, wenn die Wischfilmverdampfer (3, 4) und der Knetreaktor (9) bei unterschiedlichen Vakuumqualitäten arbeiten, vorzugsweise ist der Vakuumdruck des Knetreaktors (9) geringer als der Druck der Wischfilmverdampfer (3, 4).
  14. Verfahren nach Anspruch 1 oder Anspruch 3, wobei die Verdampfung des Materials unter Vakuum die Kondensation des verdampften Wasserdampfes durch einen Kondensator erfordert, wobei die berechnete Menge an kondensiertem Wasser und die tatsächliche Menge an kondensiertem Wasser verwendet werden, um die Temperatur des Mantelwärmemediums oder die Rotorgeschwindigkeit oder die Qualität des Vakuums oder eine Kombination zur Steuerung des Ausmasses der Feuchtigkeitsverdampfung in der Spinnmasse einzustellen, wobei, wenn die tatsächliche Kondensationsmenge kleiner als die für die Berechnung erforderliche Kondensationsmenge ist, diese durch Erhöhung der Temperatur des Wärmemediums oder Erhöhung der Drehzahl des Rotors oder Senkung des Vakuumdrucks oder durch Verwendung durch eine Kombination der vorgenannten Massnahmen eingestellt werden kann.
  15. System mit mindestens zwei vertikalen Wischfilmverdampfern (3, 4), die mit einem einzigen horizontalen, vorzugsweise zylindrischen, Knetreaktor (9) verbunden sind.
EP20736252.6A 2019-06-20 2020-06-15 Vorbereitungsmethode und vorrichtung zur herstellung von recycling-faserspinnlösungen unter verwendung der lösungsmittelmethode Active EP3987088B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102019116736.1A DE102019116736B4 (de) 2019-06-20 2019-06-20 Herstellungsverfahren und Vorrichtung zur Herstellung einer Spinnlösung aus Recyclingfasern unter Verwendung des Lösungsmittelverfahrens
PCT/EP2020/066452 WO2020254232A1 (en) 2019-06-20 2020-06-15 Preparation method and device for producing recycled fiber spinning solution using solvent method

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EP3987088A1 EP3987088A1 (de) 2022-04-27
EP3987088C0 EP3987088C0 (de) 2023-07-26
EP3987088B1 true EP3987088B1 (de) 2023-07-26

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US (1) US20220316095A1 (de)
EP (1) EP3987088B1 (de)
JP (1) JP2022537998A (de)
KR (1) KR20220024772A (de)
CN (1) CN114174571A (de)
BR (1) BR112021025681A2 (de)
CA (1) CA3144104A1 (de)
DE (1) DE102019116736B4 (de)
ES (1) ES2961515T3 (de)
WO (1) WO2020254232A1 (de)
ZA (1) ZA202200726B (de)

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DE102021100475A1 (de) * 2021-01-13 2022-08-04 List Technology Ag Dünnschichtverdampfer und Verfahren zur Herstellung eines Transfergemisches
CN113388897B (zh) * 2021-06-29 2022-06-10 北京三联虹普新合纤技术服务股份有限公司 一种大容量Lyocell纤维素原液及其连续制备工艺
TW202348633A (zh) * 2022-01-31 2023-12-16 瑞士商Ｌｉｓｔ技術股份公司 使用乾溶解法將起始材料加工為成型溶液的設備和方法
EP4219567A1 (de) * 2022-01-31 2023-08-02 LIST Technology AG Anlage und verfahren zur verarbeitung eines ausgangsmaterials zu einer formlösung nach dem trockenlöseverfahren

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WO1996030410A1 (de) 1995-03-31 1996-10-03 Akzo Nobel N.V. Verfahren zur herstellung von celluloselösungen in wasserhaltigen tertiären amin-n-oxiden
KR100575388B1 (ko) * 2004-12-30 2006-05-03 주식회사 효성 고균질 셀룰로오스 용액 및 이로 부터 제조된 섬유
CN101280476B (zh) * 2008-05-23 2010-04-14 宜宾丝丽雅集团有限公司 一种溶剂法纤维生产中nmmo溶剂的回收方法
TW201240721A (en) * 2011-04-01 2012-10-16 Acelon Chem & Fiber Corp Energy-efficient N-methylmorpholine-N-oxide solvent recycling method
DE102012103296A1 (de) * 2012-04-17 2013-10-17 List Holding Ag Verfahren zur Herstellung von Formkörpern
BR112016006237A2 (pt) * 2013-10-04 2017-08-01 List Holding Ag processo para a produção de objetos moldados
CN105536277B (zh) * 2016-03-14 2017-11-21 许达人 一种纤维素溶剂nmmo水溶液的蒸发浓缩工艺及装置

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JP2022537998A (ja) 2022-08-31
EP3987088C0 (de) 2023-07-26
DE102019116736A1 (de) 2020-12-24
EP3987088A1 (de) 2022-04-27
ES2961515T3 (es) 2024-03-12
CN114174571A (zh) 2022-03-11
DE102019116736B4 (de) 2022-03-24
KR20220024772A (ko) 2022-03-03
ZA202200726B (en) 2022-08-31
CA3144104A1 (en) 2020-12-24
BR112021025681A2 (pt) 2022-03-03
US20220316095A1 (en) 2022-10-06
WO2020254232A1 (en) 2020-12-24

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